Processing of cellulose fiber



, 1932- M. o. scHUR ET Al.

PROCESSING' OF CELLULOSE FIBER Mart-:h 1

original' Filed Aug. 10, 1927 Patented Mar. 1, 1932 UNITED STATES PATENT OFFICE MILTON O. SCHUR AND ROYAL H. RASCH, F BERLIN, NEW HAMPSHIRE, ASSIGNORS TO BROWN COMPANY, OF BERLIN, NEW HAMPSHIRE, A CORPORATION OF .MAINE PROCESSING 0F CELLULOSE FIBER Original application led August 10, 1827, Serial 110.212,000', now Patent No.` 1,730,387. Divided and this application led August 8, 1928. Serial' No. 298,240.

This invention relates to a processing of cellulose ber particularly intended to prof ties are converted lalong with the cellulose into reaction products which not only impair the stability of the derivatives but also impart a certain amount of "color thereto. The resinous matter is usually presentv to the extent of about 0.5% to 0.8% in bleached sulphite pulp, to the extent of about 0.2% to 0.4% in wood pulp rened to high alpha cellulose content, and to about the same extent in cotton. When these impurities are removed from the ber, not only is its color stability greatly enhanced, but cellulose derivatives prepared from such ber are improved to an important and surprising degree, both in stability and in freedom from color. The deresinied ber is hence more suitable for use as a raw material for `the manufacture of paper and for the production of rayon and other synthetic cellulose products, where purity of the raw material is of great moment.

In accordance with the' present invention, the resinous impurities, including resins, gums, waxes, fats and oils, are removed from the ber by extraction with organic solvents, such as alcohol, ether, chloroform, and the like. When thus extracted, the ber becomes more stable toward heat and light, and yields derivatives of greatly enhanced quality. When wood ber, in addition to being extracted, is refined to high alpha cellulose content, it yields derivatives as stable and Ias free from coloring matter as those prepared from high grade cotton. The process of the present invention, while applicable to cellulose ber derived from various sources, is hence particularly advantageous in the case of wood ber refined to high alpha cellulose content and intended to serve as a cotton ber substitute in the production of high grade papers and cellulose derivatives.

. A rened ber may be produced by treatlng raw pulp, such as sulphite, with chlorine water, digesting the chlorine-treated pulp in an alkaline liquor, and bleaching the digested product. Treatment with chlorine effects a reaction upon ligneous matter in the pulp. Alkaline digestion effects a reaction-upon and solution of chlorinated lignins, beta and gamma celluloses, resinous matter, and other non-alpha cellulose components in the pulp, so that the digested pulp is of high alpha cellulose content, requiring relatively little bleach to attain high whiteness. The resulting rened pulp, however, still contains residual resinous impurities which impair its quality. In accordance with the present invention, the pulp is subjected to extraction with an organic solvent at one or more stages of the rening process to remove these impurities. It is usually more expedient to extract the nished or bleached rened pulp, so that the extracting operation will be the last chemical treatment accorded thereto before -such pulp is, for instance, nalll,v run over a drier and formed into drier sheets, so called, or sheeted into thin papers or tissues suitable for nitration or other esterifying operation. e

The present invention has to do more particularly with a method of handling and ex tracting the ber in the form of an aqueous suspension of pulp. According to our method. extraction is effected while the suspension is being passed through and its water content rst displaced with solvent and then -with water in continuous countercurrent flow from the water by fractional distillation. It c also possesses the advantage of enabling a continuous and economical handlmg of large amounts of ber.

On the accompanying drawing, l The iigure represents diagrammatically and conventionally apparatus intended for' centration from the intermediate portion toy substantially only water at the other end, is maintained in the apparatus. Water is continuously fed into one end Vof the apparatus, and a flow of solvent is produced from bath to bath toward the other end from which water is discharged and into which pulp to be extracted is continuously fed in countercurrent iow to the water. A volume of solvent is continuously withdrawn from the apparatus at the desired point to prevent the concentration of coloring impurities in the solvent, and suiiicient fresh solvent to make up losses and to replace solvent being lWithdrawn is continuously introduced into the intermediate portion of the apparatus.

As shown in the figure, the apparatus comprises a series of sections, each consisting of a storage tank containing a pool of solvent and an extracting tank associated therewith and located thereabove. The solvent in the successive storage tanks flows in a direction opposite to the flow of the fiber. These tanks are indicated at 21, 22, 23, 24, 25, 26, 27, 28 29, and 30, in the direction of solvent iow. The solvent overflows a series of partitions -31 placed between the tanks and gradually decreasing in height from the tank`21` to the tank 30, so that substantially continuous flow of solution from the tank 21 to the tank 30 results. The extracting tanks are designated as 21a, 22a, 23a, 24a, 25a, 26a, 27a, 28a, 29a, and 30a, in the direction of flow of fiber. Each treating tank is divided into two compartments. First, there is a thickening compartment 32, in which rotates a. straining cylinderv 33, on which fiber is deposited and through which the solvent passes and is returned by a pipe 34 to the corresponding storage tank. The fiber deposited on the straining cylinder is squeezed and thickened by a press roll 35 bearing against the cylinder. The fiber is removed'from the cylinder and deposited in an agitating compartment 32a containing the solvent, by a scraper or doctor 36 acting against the cylinder and stationed,

on a partition-37 serving to divide the thickening and agitating compartments. A supply of solventis maintained in each extraction tank by withdrawing solvent from the corresponding storage tank by a pump 370, and delivering it through a pipe 38 into the agitating compartment. The fiber is agitated in the solution maintained in the extracting compartment by a pair of agitators 380, and iows over a partition 39 into the nextadjacent thickening compartment. There is thus a constant circulation of the solvent from each storage tank, through the agitating compartment of the extracting tank, and thence through the straining cylinder back to its storage tank.

The pulp is introduced into the first extracting tank 21a'through a pipe 42, and after extraction is Withdrawn at the other end of the apparatus from the extracting tank 30a through a pipe 43. The solvent is introduced into the 'extracting tank 25a through a pipe 45, and water is introduced into the storage tank 21 through a pipe 44 and Withdrawn from the storage tan 30 through a pipe 46.l

extracting tank 30a, the solvent is substanp tially entirely displaced by water.

Operation may be initially commenced by maintaining the volume of solvent continuously delivered into the extracting tank 25a, and the volume of water continuously introduced into the storage tank 21 substantially equal to the volume of Water associated with the raw fiber. The apparatus is controlled to discharge a fiber having a water content equal to that of the raw fiber, substantially only Water, therefore, being discharged through the outlet pipe 46. After the equilibrium concentration of solvent has been attained in the tanks, only sutlcient solvent to make up for the solvent bled off from the storage tank 25 through a valved pipe 49 and to make up losses need be introduced into the extracting tank 25a. The volume of Water introduced into the storage tank 21 is the'n maintained substantially equal to the Water content of the raw fiber as it is introduced, and the water discharged through the outlet pipe 46, so that the concentration of solvent in each of the storage and extracting tanks remains substantially constant during the continuous operation' of the apparatus. The flow bled olf through the pipe 49 is regulated to provide for the withdrawal of suliicient solvent to prevent accumulation of extracted matter in the apparatus. This bled-oli' solvent may be evaporated for the recovery of its valuable solvent content.

The process of extraction may be considered as comprising two steps, during both of which steps an extraction ot material from the fiber by the solvent is effected. First, the gradual displacement of the Water content of the fiber by solvent occurs, and then the gradual displacement of the solvent by Water. Consequently, substantially all the solvent except that drawn oii' through the bleed pipe 49 is maintained Within the apparatus, .substantially only Water accompanying the extracted ber discharged through the pipe 43 at one end of the apparatus. and substantially only Water beingdischarged through the outlet pipe 46 at the opposite end thereof. If the treatment is carried out at an elevated temperature, as by introducing low pressure steam into the central pool maintained in the storage tank 26, the heat content, except for that of the bleed solution and that lost due to evaporation of solvent, is maintained Within the apparatus. The counter-current process thus described may be approximated in .simpler apparatus through the use of tanks or centrifuges piped to alloW'the countercurrent displacement of Water or of solvent in the stock. y

Where an inert solvent is employed, it `may be advantageous to add other chemicals to effect a removal of impurities other than resinous from the liber. Thus, a certain amount ofchlorine may be added to a solvent such as carbon tetrachloride to remove residual li gnin. To a solvent such as alcohol, for example, a small quantity of caustic soda may be added to remove beta and gamma celluloses and other non-alpha cellulose components carried bv the fiber. Alone or in addition to the caustic soda, soap may be added. Soap aids in the removal of resinous impurities, as it tends to disperse them and also has a detergent effect upon specks present inthe fiber.

A process such as described makes possible the use of liber quite high in resinous impurities, for such fiber may be deresiniiied to a point Where it is quite suitable for the manufacture oit' high` grade papers and derivatives. Our process, therefore, permits the use of highly resinous Woods in the production of pulp, for resinous impurities surviving the liber-liberating process or subsequent chemical treatments may be satisfactorily removed.

Having thus described certain embodiments of this invention, it should be evident to those skilled in the art that various changes and modifications might be made therein Without departing from the spirit or scope of invention as deiined by the appended claims.

So tar as subject matter is concerned, this application is a division of our application Seriell No. 212,000, filed August 10, 1927, noviT Patent No. 1,730,387, oct. s, 1929.

What We claim is l. A process of extracting resinous impurities from an aqueous suspension of cellulose fiber with .a Water-miscible organic solvent of such impurities, Which comprises displacing the Water content of .said suspension With solvent and then With Water.

2. A process of extracting resinous impurities trom'an aqueous suspension of cellulose fiber with a Water-miscible organic solvent of such impurities, which comprises gradually displacing the Water content of said suspension with solvent of progressively increasing strength, and then gradually displacing the solvent content of said .suspension with solvent of progressively decreasing strength.

8. A process of extracting resinous impuri ties from cellulose pulp With a Water-miscible organic solvent of such impurities, which comprises maintaining a series of solvent baths, introducing bulk pulp into an end bath, passing said pulp from bath to bath toward the other end bath, introducing Wa.- ter into the other end bath and the solvent into an intermediate bath, and producing a iioW of water from bath to bath in countercurrent flow to that of the pulp.

4. A process of extracting resinous impurities from cellulose pulp With al Water-miscible organic solvent oi' such impurities, which comprises maintaining a series of solvent baths gradually increasing in concentration of solvent from substantially only Water at one end of the series toward an intermediate bath thereotl and gradually decreasing in concentration from the intermedi atc bath to substantially only Water at the other end thereof, introducing bulk pulp into an end bath'and passing the pulp from bath to bath toward the other end bath, introducing Water into the other end bath and solvent into the intermediate bath, and ,producing a flow of Water from bath to bath in countercurrent iow to that of the pulp.

In testimony whereof We have aliixed our signatures.

MILTON O. SCHUR. ROYAL H. RASCH. 

